WO2008007469A1 - Fluide de revêtement, film mince conducteur formé à partir du fluide de revêtement, et procédé de formation de ce dernier - Google Patents

Fluide de revêtement, film mince conducteur formé à partir du fluide de revêtement, et procédé de formation de ce dernier Download PDF

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Publication number
WO2008007469A1
WO2008007469A1 PCT/JP2007/051618 JP2007051618W WO2008007469A1 WO 2008007469 A1 WO2008007469 A1 WO 2008007469A1 JP 2007051618 W JP2007051618 W JP 2007051618W WO 2008007469 A1 WO2008007469 A1 WO 2008007469A1
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WIPO (PCT)
Prior art keywords
thin film
conductive thin
coating
chemical formula
film
Prior art date
Application number
PCT/JP2007/051618
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English (en)
Japanese (ja)
Inventor
Christopher Cordonier
Tetsuya Shichi
Takafumi Numata
Kenichi Katsumata
Akimasa Nakamura
Yasuhiro Katsumata
Teruo Komine
Kenichirou Amemiya
Makoto Yamashita
Akira Fujishima
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Central Japan Railway Company
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Central Japan Railway Company filed Critical Central Japan Railway Company
Priority to JP2008524721A priority Critical patent/JP5226512B2/ja
Priority to KR1020087030716A priority patent/KR101086921B1/ko
Priority to CN2007800265227A priority patent/CN101490309B/zh
Priority to US12/226,827 priority patent/US8003219B2/en
Priority to EP20070707804 priority patent/EP2045359A1/fr
Priority to PCT/JP2007/063929 priority patent/WO2008007751A1/fr
Priority to US12/307,725 priority patent/US8445118B2/en
Priority to EP20070790723 priority patent/EP2048111A1/fr
Priority to KR1020097002515A priority patent/KR101075285B1/ko
Priority to JP2008524846A priority patent/JP5243248B2/ja
Priority to CN2007800265212A priority patent/CN101489920B/zh
Priority to TW96125367A priority patent/TWI389987B/zh
Publication of WO2008007469A1 publication Critical patent/WO2008007469A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/066—Zirconium or hafnium; Oxides or hydroxides thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0215—Coating
    • B01J37/0219—Coating the coating containing organic compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14—Methods for preparing oxides or hydroxides in general
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
    • C09C1/3607—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/1208—Oxides, e.g. ceramics
    • C23C18/1216—Metal oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1225—Deposition of multilayers of inorganic material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1279—Process of deposition of the inorganic material performed under reactive atmosphere, e.g. oxidising or reducing atmospheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31678—Of metal

Definitions

  • the present invention relates to a coating liquid used for forming a conductive thin film, a conductive thin film, and a method for forming the same.
  • Conductive thin films are applied in a wide range of fields, and most display devices such as plasma displays (PDPs), liquid crystal displays (LCDs), and organic EL displays (O LEDs), especially in display-related applications. It has become indispensable to.
  • PDPs plasma displays
  • LCDs liquid crystal displays
  • O LEDs organic EL displays
  • liquid phase method As a method for solving these problems, there is a liquid phase method shown below. According to the liquid phase method, there is an advantage that a large apparatus is not required and energy consumption is low.
  • Patent Document 1 JP-A-6-119816
  • Patent Document 2 Japanese Unexamined Patent Publication No. 2006-73267
  • Patent Document 3 Japanese Patent Application Laid-Open No. 10-237078
  • Patent Document 4 Japanese Patent Laid-Open No. 2002-42583
  • the adhesion to the substrate may be poor and may peel off, or a large number of cracks may enter even if the substrates are in close contact.
  • the occurrence of fine cracks leads to an increase in turbidity (haze), which is not preferable for practical use.
  • the problem of cracks and adhesion is particularly noticeable when a thick film is formed. Therefore, it is necessary to strictly control the film thickness in order to obtain a good film.
  • the present invention has been made in view of these problems, and an object thereof is to provide a technique related to a conductive thin film having high adhesion to a substrate having high transparency and conductivity.
  • the gist is a coating solution that reacts with a ligand represented by Chemical Formula 1 and contains indium (In), tin (Sn), or indium (In) and tin (Sn), and both metal materials.
  • a ligand represented by Chemical Formula 1 contains indium (In), tin (Sn), or indium (In) and tin (Sn), and both metal materials.
  • R 1 to R 5 in Chemical Formula 1 are each one of the following (1) to (11):
  • X is a complex or a carboxylic acid.
  • a conductive thin film can be formed on the surface of the substrate.
  • the coating liquid of the present invention when the coating liquid of the present invention is applied to the surface of a substrate, the surface of the substrate contains indium (hereinafter also referred to as In), tin (hereinafter also referred to as Sn), or both In and Sn.
  • In indium
  • Sn tin
  • Sn both In and Sn.
  • a coating film containing a metal compound is formed.
  • the above metal compound is thermally decomposed, the ligand disappears, and a metal oxide thin film (conductive thin film) containing In, Sn, or both In and Sn is obtained. It is formed.
  • the conductive thin film formed using the coating liquid of the present invention has a high film density and excellent adhesion to a substrate that does not cause cracks.
  • the film density is high, so the conductivity is high.
  • the turbidity (haze) is low, so that a transparent conductive thin layer can be obtained.
  • a crack with a high film density does not occur is presumed as follows.
  • a metal material that reacts with the ligand represented by Chemical Formula 1 and contains In, Sn, or both In and Sn has a flat structure as shown in the molecular structural force represented by Chemical Formula 1. Therefore, when the coating solution is applied to the substrate surface to form a coating film, a molecular assembly structure (stacking) is formed such that the metal materials overlap each other due to the interaction between the metal materials.
  • the conductive thin film formed using the coating solution of the present invention has high hardness. Furthermore, since the conductive thin film formed using the coating liquid of the present invention is smooth and highly transparent, for example, when a conductive thin film is formed on the surface of glass, the transparency can be maintained. In addition, when a conductive thin film is formed on the surface of the mirror, the reflectance can be maintained.
  • the coating liquid of the present invention can form a durable conductive thin film without containing a binder. For this reason, the In oxide, Sn oxide, or In-Sn oxide concentration force S in the formed thin film is not thinner than the binder.
  • the action (for example, conductive action) by the oxide, Sn oxide, or In—Sn oxide is high.
  • the coating liquid of the present invention is stable and can be stored for a long time.
  • the metal oxide thin film (conductive thin film) formed using the coating liquid of the present invention has a function of a transparent conductive film.
  • the coating solution of the present invention can be easily produced.
  • an appropriate amount of catechol which is a ligand, is added to a raw material such as indium alkoxide tin chloride in an appropriate solvent, and then heated to produce an indium tin complex.
  • catechol which is a ligand
  • this indium-tin complex has a planar structure, it forms a molecular structure in which the complex molecules overlap each other in a coating and dry state (stacking). The interaction between aromatic rings also contributes to this molecular structure.
  • the metal material that reacts with the ligand represented by Chemical Formula 1 and contains In, Sn, or both In and Sn is, for example, an organometallic complex represented by Chemical Formula 2 or Chemical Formula 3.
  • R 1 to R 5 in Chemical Formula 2 and Chemical Formula 3 are any of (1) to (: 11) in claim 1
  • X ⁇ is a complex or a carboxylic acid.
  • the coating solution of the present invention may be used as a solvent, for example, alcohols (eg, methanol, ethanol, 2_propanol, n-butanol, isobutanol), ethers (eg, diethyl ether, MTBE, THF).
  • alcohols eg, methanol, ethanol, 2_propanol, n-butanol, isobutanol
  • ethers eg, diethyl ether, MTBE, THF.
  • Ethylene glycol monomethylol ether of ethylene glycol, dimethyl ether of ethylene glycol, hydrocarbons (eg octane, n-hexane, cyclohexane, benzene, toluene, xylene), dimethyl sulfoxide (DMSO), amides (eg dimethyl Formamide), ratatas (for example, N-methinole pyrrolidineone (NMP)), halides (for example, carbon tetrachloride, chloroform, dibutyl methane, dichloromethane), ketones (for example, acetone, methyl ethyl ketone ( MEK)), ⁇ -ketones (eg, acetyl) Luacetone (acac)), esters (for example, ethyl acetate), latatones (for example, ⁇ -petit-mouth ratataton, force prolatatone), nitroalkane
  • the concentration of the organometallic complex in the coating solution is not particularly limited as long as it does not exceed the solubility of the organometallic complex.
  • a concentration of 0.1 ⁇ to 0.8 ⁇ is suitable.
  • the corresponding organometallic complex can be used in the desired ratio.
  • the second invention of the present application is:
  • a gist of the method for forming a conductive thin film characterized in that
  • the conductive thin film formed according to the present invention has excellent adhesion to a substrate where cracks do not occur, and has high hardness. Further, as described above, since no crack is generated, the thickness of the conductive thin film can be increased.
  • the conductive thin film formed according to the present invention is hard and smooth and has high transparency, for example, when a conductive thin film is formed on the surface of glass, the transparency can be maintained. When the conductive thin film is formed on the surface of the mirror, the reflectance can be maintained.
  • the coating liquid used in the present invention can form a durable conductive thin film even if it does not contain a binder. Therefore, In oxide and Sn oxidation in the formed thin film Indium oxide, Sn oxide, or In-Sn oxide has a high effect (for example, conductive effect).
  • the substrate is not particularly limited, but when a firing method is used in the step of forming the conductive thin film, it is desirable that the substrate be a substance that can withstand the temperature during firing.
  • Specific examples of the substrate include, for example, heat resistance of glass (for example, PYREX (registered trademark) glass, ordinary glass, quartz glass), ceramics (for example, alumina, zirconia, silica), and resin (for example, polyimide resin). Examples include polymers.
  • a wet method that can form a coating film of a coating solution can be used widely. Force that can be used S For example, spin coating, dip coating, spray coating, and other commonly used coatings A method is mentioned. In addition, it is preferable to dry the coating film naturally under normal temperature and pressure after applying the coating solution. Thereafter, for example, the coating film can be baked.
  • a method of changing the organometallic compound into a conductive thin film for example, there is a method of baking a coating film formed by applying a coating liquid.
  • the firing temperature is preferably in the range of 350 to 1000 ° C, for example.
  • the firing temperature is 350 ° C or higher, a dense film can be formed, so that a conductive thin film having conductivity and transparency can be obtained. Furthermore, when the firing temperature is 700 ° C. or higher, a dense film can be formed, and thus a transparent conductive thin film with higher conductivity can be obtained.
  • a conductive thin film having a lower resistivity when the firing is performed in the air and further in a reducing atmosphere (for example, in a mixed gas atmosphere of nitrogen and hydrogen), a conductive thin film having a lower resistivity can be formed. .
  • the firing temperature may be as low as about 350 ° C.
  • the conductive thin film can be formed on the surface of the substrate that is vulnerable to heat by using the coating liquid of the present invention. it can. Further, even when the substrate is made of ordinary glass, a conductive thin film can be formed without an undercoat.
  • the firing temperature can be adjusted according to the type of metal M and the desired crystalline phase of the conductive thin film.
  • the third invention of the present application is:
  • the conductive thin film formed by the method for forming a conductive thin film according to the second invention is The gist.
  • the conductive thin film of the present invention has high hardness without generating cracking force, and excellent adhesion to the substrate. Furthermore, since the conductive thin film of the present invention is smooth and highly transparent, for example, when a conductive thin film is formed on the surface of glass, the transparency can be maintained, and the surface of the mirror is electrically conductive. When the conductive thin film is formed, the reflectance can be maintained.
  • the conductive thin film of the present invention does not need to contain a binder, it is thinner than the concentration power binder of In oxide, Sn oxide, or In-Sn oxide in the formed thin film.
  • the action of In oxide, Sn oxide, or In-Sn oxide is high.
  • the fourth invention of the present application is:
  • the gist of the present invention is a conductive thin film-coated product comprising a substrate and the conductive thin film formed on the surface of the substrate according to the second invention.
  • the conductive thin film-coated product of the present invention is excellent in adhesion to a substrate having a high hardness S and a crack S. Furthermore, since the conductive thin film in the present invention is smooth and highly transparent, for example, the transparency can be maintained when the substrate is glass, and the reflectance is increased when the substrate is a mirror. Can be maintained. In addition, since the conductive thin film in the present invention does not need to contain a binder, it is thinner than the concentration power binder of In oxide, Sn oxide, or In-Sn oxide in the formed thin film. The action (for example, conductive effect) by In oxide, Sn oxide, or In-Sn oxide is high.
  • the substrate is not particularly limited, but when a firing method is used in the conductive thin film formation step, the substrate is preferably a substance that can withstand the temperature during firing.
  • Specific examples of the substrate include, for example, heat resistance of glass (for example, PYREX (registered trademark) glass, ordinary glass, quartz glass), ceramics (for example, alumina, zirconia, silica), and resin (for example, polyimide resin). Examples include polymers.
  • FIG. 1 is an explanatory diagram showing the molecular structure of an iminodiethanol complex.
  • the solid content did not change even when stored for 6 months or longer. Even after coating 6 months or longer after synthesis, the sample did not change in electrical and optical characteristics from the sample produced immediately after synthesis.
  • Example 1 Dissolve the powders obtained in Example 1 and Example 2 shown in Table 1 in a mixture of 5 mL of acetylacetone and toluene at a ratio shown in Table 2 below, and apply a metal ion concentration of 0.5M. A liquid was obtained. [0058] 0.4 mL of the solution was coated on a quartz glass plate (50 X 50 X 2 t mm) by spin coating (rotation speed at the time of application: 750 ⁇ ⁇ ⁇ ). Thereafter, the coated glass substrate was baked at 900 ° C. for 1 hour (temperature rising 10 ° C. min min, natural cooling) to obtain a conductive thin film. Table 2 shows the sheet resistance, total transmittance, and turbidity of the formed conductive thin film.
  • Example 3 Based on the above results, the amounts shown in Table 3 below were added to a solution prepared by mixing the powder of Example 3 shown in Table 1 prepared in Table 1 with the optimum values of In and Sn precursors in a 1: 1 mixture of lOOmL of acetylacetone and toluene. Dissolved to obtain a coating solution.
  • the coating solution is free from precipitation even after 4 months. It was chemically stable and could be used in the same manner as immediately after production.
  • Annealing was performed at ° C for 1 hour (temperature increase 10 ° C Zmin, natural cooling) (Example 11_4A).
  • Table 3 shows the composition of the coating solution before firing, the film thickness and resistivity after firing, sheet resistance, total transmittance, turbidity and film hardness.
  • the sheet resistance and resistivity of the conductive thin film were measured using NPS resistance measuring instrument IV-5 (using KS-TC-40-TF-VR probe) based on JIS R 1635.
  • the total transmittance and turbidity were Nippon Denshoku Industries Co., Ltd. NDH5000W was used and measured based on JIS Z 8722.
  • the film thickness is measured by measuring the absorption of the substrate at a light wavelength of 250 nm with a spectrophotometer (Hitachi U-3310), confirming the corresponding film thickness with SEM (Hitachi S-4800), and using the following formula The coefficient was obtained.
  • the hardness measurement conditions were in accordance with the pencil grabbing test (JIS K 5400).
  • the film thickness changed in proportion to the solid content concentration of the coating solution.
  • the film hardness was as high as> 9H even when the film thickness was large.
  • the resistivity Both the gate resistance decreased. Annealing further lowered the resistivity and sheet resistance.
  • Example 3 An appropriate amount of the powder obtained in Example 3 shown in Table 1 was dissolved in a 5: 1 solution of 5 mL of acetylacetone and toluene to obtain a coating solution having a metal ion concentration of 0.75M. 0.4 mL of the solution was coated on a quartz glass plate (50 ⁇ 50 ⁇ 2 tmm) by spin coating (rotation speed at coating: 750 rpm). Thereafter, the coated glass substrate was baked for 1 hour in the range of 350 to 1000 ° C. (temperature increase 10 ° C. Zmin, natural cooling) to obtain a conductive thin film. Table 4 shows the resistivity and sheet resistance of the formed conductive thin film.
  • Example 3 An appropriate amount of the powder obtained in Example 3 shown in Table 1 was dissolved in a solution of 5 mL of acetylacetone and toluene mixed 1: 1 to obtain a coating solution having a metal ion concentration of 0.25M. 0.4 mL of the solution was coated on a quartz glass plate (50 ⁇ 50 ⁇ 2 tmm) by spin coating (rotation speed at coating: 750 rpm). Thereafter, the coated glass substrate was baked at 900 ° C. for 1 hour (temperature increase: 10 ° C./min, natural cooling) to obtain a conductive thin film. Then, the resistivity, sheet resistance and optical properties, and film hardness of the conductive thin film were measured, and the coating process and firing were repeated five times.
  • Example 13-5A The sample with the lowest resistivity was fired and then annealed in a reducing atmosphere at 500 ° C for 1 hour (temperature increase 10 ° C / min, natural cooling) (Example 13-5A).
  • Table 5 shows the resistivity, sheet resistance, and optical characteristics of the formed conductive thin film.
  • the film hardness was as high as 9mm. At the same time, the resistivity and sheet resistance decreased as the film thickness increased. There was almost no change in optical properties.
  • Example 3 to Example 9 shown in L were dissolved in the solvent shown in Table 6 in the amount shown in Table 6 to obtain a coating solution having a metal ion concentration of 0.25 kg. Then, 0.4 mL of the solution was coated on a quartz glass plate (50 ⁇ 50 ⁇ 2 tmm) by spin coating (rotation speed at coating: 750 rpm). Thereafter, the coated glass substrate was baked at 900 ° C. for 1 hour (temperature increase 10 ° C. Zmin, natural cooling) to obtain a conductive thin film. Then, the resistivity, sheet pile and optical properties of the conductive thin film were measured.
  • Example 9 8.68 24 15 6733 90 0.26 From the above results, the conductivity and transparency of the substrate were confirmed even when the solvent or ligand was other than Example 3 shown in Table 1.
  • Table 8 shows a comparison between examples and comparative examples depending on the ligand. All samples were coated with a 0.5M solution.
  • the refractive index when the wavelength of light is 550 nm is measured with an ellipsometer (Mizojiri Kogyo DHA—XAV W / S6), and the porosity of the film is calculated by the following equation. Asked. Table 9 below shows the comparison.
  • Example 1 1 1 3 1.777 13.2% 3.7 Ratio «Example 4 1 3 1.487 56.7% 29.4 From the above, it can be seen that in the examples, the membrane is denser (porosity is low) and the resistivity is also low.
  • Table 10 shows a comparison between the case where the coating solution with low concentration is repeatedly applied and baked, and the case where the coating solution with high concentration is applied.

Abstract

L'invention concerne un fluide de revêtement contenant une matière métallique qui réagit avec un ligand représenté par le 1,2-benzènediol, la phénylènediamine, le 2-aminophénol, le 2-aminothi-phénol, l'acide anthranilique, l'acide salicylique, l'acide thiosalicylique, etc., et comprend l'indium (In), l'étain (Sn) ou à la fois l'indium (In) et l'étain (Sn). L'invention concerne également un procédé de formation d'un film mince conducteur qui comprend l'application du fluide de revêtement sur une surface de base afin de former un film de revêtement et la cuisson de celui-ci pour ainsi transformer le ou les éléments choisis dans le groupe constitué par les matières métalliques et contenus dans le film de revêtement en film mince conducteur; et un film mince conducteur obtenu par le procédé de fabrication. Le film mince conducteur peut avoir une transparence élevée et une conductivité élevée et présenter une adhérence élevée à la base.
PCT/JP2007/051618 2006-07-13 2007-01-31 Fluide de revêtement, film mince conducteur formé à partir du fluide de revêtement, et procédé de formation de ce dernier WO2008007469A1 (fr)

Priority Applications (12)

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JP2008524721A JP5226512B2 (ja) 2006-07-13 2007-01-31 塗布液、塗布液を用いて形成した導電性薄膜、およびその形成方法
KR1020087030716A KR101086921B1 (ko) 2006-07-13 2007-01-31 도포액，도포액을 이용하여 형성한 도전성 박막，및 그 형성방법
CN2007800265227A CN101490309B (zh) 2006-07-13 2007-01-31 涂布液、使用涂布液形成的导电性薄膜及其形成方法
US12/226,827 US8003219B2 (en) 2006-07-13 2007-01-31 Coating liquid, conductive film formed by coating liquid, and forming method thereof
EP20070707804 EP2045359A1 (fr) 2006-07-13 2007-01-31 Fluide de revêtement, film mince conducteur formé à partir du fluide de revêtement, et procédé de formation de ce dernier
PCT/JP2007/063929 WO2008007751A1 (fr) 2006-07-13 2007-07-12 Liquide de revêtement, couche mince de composé métallique formée en utilisant le liquide de revêtement et son procédé de formation
US12/307,725 US8445118B2 (en) 2006-07-13 2007-07-12 Coating liquid, metal compound film formed by coating liquid, and forming method thereof
EP20070790723 EP2048111A1 (fr) 2006-07-13 2007-07-12 Liquide de revêtement, couche mince de composé métallique formée en utilisant le liquide de revêtement et son procédé de formation
KR1020097002515A KR101075285B1 (ko) 2006-07-13 2007-07-12 도포액, 도포액을 이용하여 형성된 금속화합물박막 및 그 형성방법
JP2008524846A JP5243248B2 (ja) 2006-07-13 2007-07-12 塗布液、及び金属化合物薄膜の形成方法
CN2007800265212A CN101489920B (zh) 2006-07-13 2007-07-12 涂布液、使用涂布液形成的金属化合物薄膜及其形成方法
TW96125367A TWI389987B (zh) 2006-07-13 2007-07-12 A coating liquid, a metal compound film formed by using a coating liquid, and a method for forming the same

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JP2006-193415 2006-07-13

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PCT/JP2006/325783 WO2008007453A1 (fr) 2006-07-13 2006-12-25 Liquide de revêtement, couche mince d'oxyde de titane formée en utilisant le liquide de revêtement et son procédé de formation
PCT/JP2007/051618 WO2008007469A1 (fr) 2006-07-13 2007-01-31 Fluide de revêtement, film mince conducteur formé à partir du fluide de revêtement, et procédé de formation de ce dernier
PCT/JP2007/063929 WO2008007751A1 (fr) 2006-07-13 2007-07-12 Liquide de revêtement, couche mince de composé métallique formée en utilisant le liquide de revêtement et son procédé de formation

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PCT/JP2006/325783 WO2008007453A1 (fr) 2006-07-13 2006-12-25 Liquide de revêtement, couche mince d'oxyde de titane formée en utilisant le liquide de revêtement et son procédé de formation

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CN101484387A (zh) 2009-07-15
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KR101025122B1 (ko) 2011-03-25
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US7964283B2 (en) 2011-06-21
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US8445118B2 (en) 2013-05-21
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